CN112090106B - Reagent purification device and method for purifying ammonium bifluoride or ammonium fluoride by using same - Google Patents
Reagent purification device and method for purifying ammonium bifluoride or ammonium fluoride by using same Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
- B01D7/02—Crystallisation directly from the vapour phase
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/162—Ammonium fluoride
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Abstract
The invention belongs to the field of analysis and detection, and particularly relates to a reagent purification device and a method for purifying ammonium bifluoride or ammonium fluoride by using the same4HF2Or NH4F vapor is crystallized in situ at different positions of the reagent collecting bottle. The purification device is of a vertical totally-enclosed structure, temperature and time parameters can be designed in advance through a program, and automatic purification is realized. Simple equipment principle, can be used by combining a plurality of units, and can purify a large amount of NH at one time4HF2Or NH4The reagent F is efficient, simple and convenient.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a reagent purification device and a method for purifying ammonium bifluoride or ammonium fluoride by using the same.
Background
The contents of main trace elements and isotope ratio information in geological samples such as rocks, sediments, soil or minerals and the like provide important geochemical information for researching major geoscience problems such as earth evolution, environmental change, deposit cause, mineral resource distribution and the like. In recent years, instruments and equipment are rapidly developed, so that the quality of element analysis and isotope composition analysis test data and the production efficiency are greatly improved. However, due to the complexity of geological samples, almost all geological samples require pretreatment of the samples in the early stage of the overall analysis and testing, and complex solid geological samples are completely converted into homogeneous and clear solutions (digestion), and the process from the basic principle to the operation mode is not significantly different from the middle of the last century. The traditional geological sample digestion technology is not only complicated in process, but also consumes a large amount of strong acid, strong alkali and other chemical reagents, and most of the chemical reagents are discharged in the form of waste gas and waste liquid. Therefore, the digestion of the geological sample not only becomes the weakest ring in the analysis process of the geological sample, but also causes serious pollution to the environment due to a large amount of discharged harmful gas and waste liquid.
In recent years, research on novel geological sample pretreatment technologies has received increasing attention. The solid reagent ammonium bifluoride (NH) originally proposed by China4HF2) Or ammonium fluoride (NH)4F) Can replace strong corrosive hydrofluoric acid (HF) to digest geological samples. The traditional geological sample pretreatment often has the problems of low digestion efficiency of indissolvable side minerals, easy formation of indissolvable fluorides and the like, and the test accuracy is influenced. In particular to aluminum-rich rock (such as bauxite, ancient weathering crust, moraine and the like), indissolvable aluminum fluoride precipitation is easy to appear by utilizing a closed high-pressure digestion method, so that the test value of the rare earth element is remarkably lower. NH (NH)4HF2Or NH4Compared with the traditional inorganic acid, the F has higher boiling point (240 ℃ and 250 ℃), the sample digestion temperature can be increased to 230 ℃ under normal pressure, the rock rich in the indissolvable accessory minerals can be completely digested within 2 hours, and the efficiency is improved by more than 20 times. NH (NH)4HF2Or NH4The F digestion method does not need a high-temperature high-pressure sealing device, is simple and convenient to operate, reduces the labor intensity and the experiment cost, avoids using HF with strong toxicity to human bodies, and greatly reduces the working risk of experimenters. NH in comparison with conventional methods4HF2Or NH4Method for digestion of FHas the advantages of high efficiency, safety, simple operation, low cost and the like.
One practical problem, however, is that of analytical grade NH purchased commercially4HF2Or NH4F (purity 99.8%) often has high transition metal elements (Co, Ni, Cu, Zn and the like), and can cause pollution to the analysis of trace elements of geological samples. Higher purity NH4HF2Or NH4F (purity 99.99%) requires a high price (500 g about 900-. Therefore, a small NH4HF2 or NH4F purification device capable of meeting the daily analysis requirements of a laboratory is designed and manufactured to develop a large amount of NH4HF2Or NH4And F, the geological sample is digested and popularized to units of geological prospecting nationwide, and the method has important significance.
Usually NH4HF2Or NH4The mode of F is sublimation purification. According to different application scenes, the design of the purification equipment is greatly different. In the field of geological sample pretreatment, NH reported in literature4HF2Or NH4The F process is a two-bottle purification designed by Zhang et al, (2012) and O' Hara et al, (2017). This method uses a bottle collector at an angle of approximately 90 degrees, and places the starting reagent on one side, which is heated by an infrared lamp or heating element. Sublimed NH4HF2Or NH4The F vapor is transferred to a cold collection bottle on the other side and crystallized to high purity NH4HF2Or NH4F. The equipment is simple in design and suitable for laboratories. But in actual use, due to NH4HF2Or NH4F has a higher boiling point, making NH4HF2Or NH4The F vapor will crystallize rapidly upon leaving the heated zone, blocking the mouth of the cold trap bottle, so that the vapor cannot eventually reach the bottom of the cold trap bottle. So the pair of bottles NH4HF2Or NH4The efficiency of the F purification device is low.
Patent CN 103566606A discloses a multifunctional purification device and a method for purifying ammonium bifluoride by using the same, and the specific principle is that NH is added4HF2Heating, then mixingNH steam4HF2Condensed into liquid, flows through a condenser tube into a collector flask, where it crystallizes into solid NH4HF2. However, in practical application, NH may occur in the technical scheme4HF2The problem of local crystallization of steam in the transmission pipeline leads to the condenser pipe jam, and the reagent can't pass through or only has a small amount of effluences, influences purification efficiency. Thus improving NH4HF2Or NH4The condensing and crystallizing position of F vapor avoids the problem of the blockage of a purified substance transmission pipeline, and is designed to be new NH4HF2Or NH4F, important improvement direction of the purifying equipment.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcome prior art's not enough, provide a reagent purification device and utilize device purification ammonium bifluoride or ammonium fluoride method, specifically adopt the mode of cooling down step by step, realize the quick purification function of ammonium bifluoride or ammonium fluoride reagent to satisfy the geological analysis laboratory and develop a large amount of NH4HF2Or NH4And F, resolving the reagent dosage requirement of the work of geological sample.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a reagent purification device can be used for purifying ammonium bifluoride or ammonium fluoride reagent, and is characterized in that: the purification device comprises a reagent heating bottle and a reagent collecting bottle, wherein heating devices are arranged along the circumferential directions of the reagent heating bottle and the reagent collecting bottle, each heating device is a heating platform with a hollow design, each heating platform comprises more than two heating holes, each heating hole can be used for placing a heating collecting bottle assembly, each heating hole is divided into more than three temperature control areas from top to bottom, and each temperature control area is controlled by an independent heater;
further, the reagent heating bottle and the reagent collecting bottle are screwed up in a knob mode through threads, and the reagent heating bottle and the reagent collecting bottle form a vertical fully-closed structure.
Further, in order to make NH4HF2Or NH4F can be preferentially crystallized in situ at the bottom of the collection bottle, and the tail part of the reagent collection bottle is higher than the heating hole.
Furthermore, the height of the collecting bottle higher than the heating hole part is specifically 25mm-50mm, namely NH can be realized4HF2Or NH4And F, gradually cooling and crystallizing the steam.
Further, the heating device comprises the heating hole, a heating module and an equipment power supply control system; a control component is arranged to control the power supply, the circuit board and the temperature control button.
Further, for practical use and simple and convenient processing and production, the reagent heating bottle and the reagent collecting bottle are straight barrel type PTFE bottles, and the reagent heating bottle and the reagent collecting bottle can be connected through thread sealing;
further, the reagent heating bottle and the reagent collecting bottle are arranged up and down;
further, in order to enlarge the surface area of the inside of the collecting bottle, NH is increased4HF2Or NH4F, the inner part of the reagent collecting bottle is of a three-layer structure, and the PTFE baffles are used for carrying out space separation;
furthermore, in order to realize simultaneous purification, more than two heating holes are arranged, and six heating holes can be specifically arranged;
further, the heating hole is divided into at least three temperature control areas from top to bottom; the temperature can be set manually or the heating mode can be set by programming;
further, the method for purifying the ammonium bifluoride or ammonium fluoride reagent according to the reagent purification device specifically comprises the following steps: (1) initial NH4HF2Or NH4F, placing the mixture in a cleaned reagent heating bottle, and filling about one third of the reagent heating bottle; (2) screwing the cleaned reagent collecting bottle and the reagent heating bottle in a knob mode, and then placing the reagent heating bottle and the reagent collecting bottle assembly into the heating hole, wherein the reagent heating bottle faces downwards, and the reagent collecting bottle faces upwards; (3) the power switch of the heating device is turned on, and all the heating modules are regulated to 230-At this time NH4HF2Or NH4F will evaporate and the vapour will move upwards and, after leaving the uppermost heating module (heating module 3.1), will rapidly crystallise at the bottom of the reagent collection vial due to the temperature drop. The reagent collecting bottle is divided into three layers by the PTFE baffle, thereby increasing the surface area in the collecting bottle and being beneficial to accelerating NH4HF2Or NH4F is crystallized; (4) after heating for a while, the temperature of the heating module 3.1 is adjusted to 0, NH4HF2Or NH4F steam is crystallized at the position of a heating module 3.1; (5) after heating for a period of time, the temperature of the heating module 3.2 is adjusted to 0, NH4HF2Or NH4F steam is crystallized at the position of a heating module 3.2; (6) heating for a period of time, turning off the power supply, cooling the reagent collecting bottle, taking out the reagent heating bottle and the reagent collecting bottle assembly, decomposing, and collecting the whole bottle of purified NH in the collecting bottle4HF2Or NH4And F, covering the reagent collecting bottle with a bottle cap for storing and using. While remaining NH4HF2Or NH4F is retained in the reagent heating bottle.
Compared with the prior art, the invention has the beneficial effects that: the invention utilizes the sub-boiling distillation phase equilibrium principle to purify ammonium bifluoride or ammonium fluoride, and NH is enabled to be integrally heated and gradually cooled4HF2Or NH4F vapor is crystallized in situ at different positions of the reagent collecting bottle. The reagent heating bottle and the reagent collecting bottle of the purification device are screwed up in a knob mode through threads, and the reagent heating bottle and the reagent collecting bottle form a vertical totally-enclosed structure. The temperature and time parameters can be designed in advance through a program, and automatic purification is realized. Simple equipment principle, can be used by combining a plurality of units, and can purify a large amount of NH at one time4HF2Or NH4The reagent F is efficient, simple and convenient.
Drawings
FIG. 1 is a schematic view of the structure of a reagent purification apparatus;
FIG. 2 is an internal structure view of the multi-functional purification apparatus;
labeled as: 1-a reagent collecting bottle, 2-a reagent heating bottle, 3-a heating device, 3.1-a heating module, 3.2-a heating module, 3.3-a heating module, 3.4-a heating module, and 4 is a control component.
Detailed Description
The invention will be further described with reference to the following examples:
referring to fig. 1-2, a reagent purification apparatus, which can be used for purifying ammonium bifluoride or ammonium fluoride reagents, the purification apparatus is a square apparatus with a length, width and height of 330mm, 220mm and 250mm, the apparatus includes a reagent collection bottle 1 and a reagent heating bottle 2, a heating apparatus 3 is arranged along the circumferential direction of the reagent collection bottle 1 and the reagent heating bottle 2, the heating apparatus 3 is a hollow heating platform, the heating platform includes six heating holes, each heating hole can be used for placing a heating reagent collection bottle assembly, the heating holes are divided into four temperature control zones from top to bottom, and each temperature control zone is controlled by an independent heater; a part of the tail part of the reagent collecting bottle is higher than the heating hole; the height of the reagent collecting bottle higher than the heating hole part is specifically 25mm-50mm, preferably 40mm; the interior of the reagent collecting bottle is of a three-layer structure, and is spatially separated by a PTFE baffle; the temperature can be set manually or the heating mode can be set by programming; NH is reduced by integral heating and gradual cooling4HF2Or NH4F vapor is crystallized in situ at different positions of the reagent collecting bottle. The purification device is of a vertical totally-enclosed structure, a control part 4 is arranged to control a power supply, and temperature and time parameters are designed in advance by a circuit board and a temperature control button, so that automatic purification is realized.
The purification method of the above apparatus will be described with reference to specific examples.
The first embodiment is as follows:
in this embodiment, the above purification apparatus is used to purify ammonium bifluoride.
(1) Initial NH4HF2The reagent heating bottle is placed in a cleaned reagent heating bottle, about one third of the reagent heating bottle is filled (about 150 g), and six reagent heating bottles (about 900 g) can be filled at a time; (2) collecting the cleaned reagent with a testThe reagent heating bottles are screwed down in a knob mode, and then the six reagent heating bottle and reagent collecting bottle assemblies are placed in the heating holes, the reagent heating bottles face downwards, and the reagent collecting bottles face upwards; (3) a power switch of the heating device is turned on, and all four heating modules are adjusted to 230 ℃ and NH4HF2The steam moves upwards and is rapidly crystallized at the bottom of the reagent collecting bottle; (4) after 20 minutes, the temperature of the heating module 3.1 is adjusted to 0, NH4HF2The steam is crystallized at the position 3.1 of the heating module; (5) after 40 minutes, the temperature of the heating module 3.2 is adjusted to 0, NH4HF2The steam is crystallized at the position of the heating module 3.2; (6) after 60 minutes, the power supply is turned off, after the reagent collecting bottle is cooled, the six reagent heating bottles and the reagent collecting bottle assembly are taken out, and at the moment, a whole bottle of purified NH is collected in the reagent collecting bottle4HF2And the reagent can be stored and used after the reagent collecting bottle is covered by the bottle cap. NH prepared in this example4HF2The content of metal ion impurities such as Li, Be, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Rb, Sr, REE, Ag, Ba, Hf, Pb, etc. is 0.001-0.15 ng g by ICP-MS detection-1Within the range.
Example two:
in this embodiment, the above purification apparatus is used to purify ammonium fluoride.
(1) Initial NH4F, placing the reagent heating bottle in a cleaned reagent heating bottle, filling about one third of the reagent heating bottle (about 150 g), and filling six reagent heating bottles (about 900 g) at a time; (2) screwing the cleaned reagent collecting bottle and the reagent heating bottle tightly in a knob mode, and then placing the six reagent heating bottle and reagent collecting bottle assemblies into the heating holes, wherein the reagent heating bottle faces downwards, and the reagent collecting bottle faces upwards; (3) a power switch of the heating device is turned on, and the four heating modules are all adjusted to 240 ℃ and NH4F, enabling the steam to move upwards and quickly crystallize at the bottom of the reagent collecting bottle; (4) after 20 minutes, the temperature of the heating module 3.1 is adjusted to 0, NH4F steam is crystallized at the position of a heating module 3.1; (5) after 40 minutes, the temperature of the heating module 3.2 is adjusted to 0, NH4F steam in the heating module3.2 position crystallization; (6) after 60 minutes, the power supply is turned off, after the reagent collecting bottle is cooled, the six reagent heating bottles and the reagent collecting bottle assembly are taken out, and at the moment, a whole bottle of purified NH is collected in the reagent collecting bottle4And F, covering the reagent collecting bottle with a bottle cap for storing and using. NH prepared in this example4The content of metal ion impurities such as Li, Be, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Rb, Sr, REE, Ag, Ba, Hf, Pb, etc. in F is 0.001-0.15 ng g by ICP-MS detection-1Within the range.
The working principle and the specific implementation mode of the invention are as follows: the invention utilizes the sub-boiling distillation phase equilibrium principle to purify ammonium bifluoride or ammonium fluoride, and NH is enabled to be integrally heated and gradually cooled4HF2Or NH4F vapor is crystallized in situ at different positions of the reagent collecting bottle. The purification device is of a vertical totally-enclosed structure, temperature and time parameters can be designed in advance through a program, and automatic purification is realized. Simple equipment principle, can be used by combining a plurality of units, and can purify a large amount of NH at one time4HF2Or NH4The reagent F is efficient, simple and convenient.
Geological sample pretreatment is an important aspect for restricting the improvement of sample analysis efficiency. For traditional geological sample solution testing methods, it is necessary that the rock powder sample be completely digested into soluble ions. The process is not only tedious and time-consuming (several days), but also consumes a large amount of chemical reagents such as acid, alkali, etc. The discharged large amount of harmful gas and waste liquid can cause serious pollution to the environment. It is estimated preliminarily that millions of tons of solids are dissolved in millions of tons of acid every year around the world, and the discharged large amount of harmful gas and waste liquid causes serious pollution to the environment. In order to separate the geological sample pretreatment technology from the traditional modes of heavy pollution, heavy consumption, low efficiency and high manual strength, the key for solving the problem is to develop the green geochemical analysis technical research of innovative concepts.
In recent years, research on novel geological sample pretreatment technologies has received increasing attention. The solid reagent ammonium bifluoride (NH) originally proposed by China4HF2) Or ammonium fluoride（NH4F) Can replace strong corrosive hydrofluoric acid (HF) to digest geological samples. NH in comparison with conventional methods4HF2Or NH4The F digestion method has the obvious advantages of high efficiency, safety, simple and convenient operation, low cost and the like. One practical problem, however, is that of analytical grade NH purchased commercially4HF2Or NH4F (purity 99.8%) often has high transition metal elements (Co, Ni, Cu, Zn and the like), and can cause pollution to the analysis of trace elements of geological samples. Therefore, the invention designs small-sized NH which can meet the daily analysis requirement of a laboratory4HF2Or NH4F, a purification device. The device specifically adopts the mode of cooling down step by step, realizes NH4HF2Or NH4And F, a rapid purification function of the reagent. The device has simple structure, convenient operation, small occupied area and no harsh requirement on the working environment, and can finish about 900 g of NH in one hour4HF2Or NH4F purification, the production efficiency and the product quality of the F purification can meet the requirement of daily geological sample NH4HF2Or NH4F, digestion and trace element analysis. This invention develops a large amount of NH4HF2Or NH4And F, the geological sample is digested and popularized to units of geological prospecting nationwide, and the method has important significance.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention should still fall within the scope of the patent coverage of the present invention without departing from the technical solution of the present invention.
Claims (1)
1. A method of purifying ammonium acid fluoride or ammonium fluoride, characterized by: the method comprises the following steps of purifying ammonium bifluoride or ammonium fluoride by using a reagent purification device, wherein the reagent purification device comprises a reagent heating bottle and a reagent collecting bottle, and the purification method specifically comprises the following steps: (1) placing the initial NH4HF2 or NH4F in a cleaned reagent heating bottle, filling approximately one third of the reagent bottle; (2) screwing the cleaned reagent collecting bottle and the reagent heating bottle in a knob mode, and then placing the reagent heating bottle and the reagent collecting bottle assembly into the heating hole, wherein the reagent heating bottle faces downwards, and the reagent collecting bottle faces upwards; (3) a power switch of the heating device is turned on, the heating modules are all adjusted to 230-240 ℃, at this time, NH4HF2 or NH4F will evaporate, vapor moves upwards, and after the heating module (3.1) at the top is separated, the vapor can be rapidly crystallized at the bottom of the reagent collecting bottle due to the reduction of temperature, the reagent collecting bottle is divided into three layers by the PTFE baffle plate, so that the surface area in the reagent collecting bottle is increased, and the crystallization of NH4HF2 or NH4F can be accelerated; (4) after heating for a while, the temperature of the heating module (3.1) is adjusted to 0, NH4HF2 or NH4F vapor is crystallized at the position of the heating module (3.1); (5) after heating for a while, the temperature of the heating module (3.2) is adjusted to 0, NH4HF2 or NH4F steam is crystallized at the position of the heating module (3.2); (6) and (3) turning off the power supply after heating for a period of time, taking out the reagent heating bottle and the reagent collecting bottle assembly after the reagent collecting bottle is cooled, decomposing the reagent heating bottle and the reagent collecting bottle assembly, collecting a whole bottle of purified NH4HF2 or NH4F reagent in the collecting bottle, covering the reagent collecting bottle with a bottle cap for storage and use, and keeping residual NH4HF2 or NH4F in the reagent heating bottle.
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| CN113358436B (en) * | 2021-06-11 | 2022-12-30 | 中国科学技术大学 | Device and method for purifying ammonium bifluoride |
| CN117303402B (en) * | 2023-11-30 | 2024-01-30 | 山东飞源东泰高分子材料有限公司 | Ammonium bifluoride refining purification device |
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